TWI660926B - 透明擴散oled基板及製造此基板之方法 - Google Patents
透明擴散oled基板及製造此基板之方法 Download PDFInfo
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- 239000000758 substrate Substances 0.000 title claims abstract description 79
- 238000004519 manufacturing process Methods 0.000 title description 3
- 210000003298 dental enamel Anatomy 0.000 claims abstract description 87
- 239000011521 glass Substances 0.000 claims abstract description 87
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 41
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 40
- 239000008188 pellet Substances 0.000 claims abstract description 39
- 238000010304 firing Methods 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 22
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims abstract description 7
- 239000011148 porous material Substances 0.000 claims description 27
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 5
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 claims description 3
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 3
- GEIAQOFPUVMAGM-UHFFFAOYSA-N ZrO Inorganic materials [Zr]=O GEIAQOFPUVMAGM-UHFFFAOYSA-N 0.000 claims description 3
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- 238000000149 argon plasma sintering Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
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- 239000001856 Ethyl cellulose Substances 0.000 description 3
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 3
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- 229910004298 SiO 2 Inorganic materials 0.000 description 2
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- 239000005361 soda-lime glass Substances 0.000 description 2
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- 230000035515 penetration Effects 0.000 description 1
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- 229920000642 polymer Polymers 0.000 description 1
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- 230000009257 reactivity Effects 0.000 description 1
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- 238000007711 solidification Methods 0.000 description 1
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Abstract
本發明關於製備用於發光裝置之層壓基板的方法,該方法包括下列連續步驟:(a)提供具有於550nm之折射率為介於1.45和1.65之間的玻璃基板(1),(b)將包含至少30重量%之Bi2O3且具有於550nm之折射率為至少1.7之玻璃粒料(3)塗覆至該玻璃基板(1),(c)在高於玻璃粒料之利托敦溫度的溫度,燒製所得之經粒料塗覆的玻璃基板,以形成第一高折射率琺瑯層(4),(d)將金屬氧化物層(2)塗覆至該第一高折射率琺瑯層,(e)在高於玻璃粒料之利托敦溫度的溫度,包括介於530℃和620℃之間,燒製所得之經塗覆的玻璃基板,以使金屬氧化物(2)與下方之第一高折射率琺瑯層(4)反應,及形成第二高折射率琺瑯層(5),其具有複數個球形孔隙(6)埋於第二高折射率琺瑯層(5)之上段中接近與空氣之界面處,以及,隨意地(f)將透明導電層(TCL)(8)塗覆於該第二高折射率琺瑯層(5)以上。
Description
本發明係關於製造用於有機發光二極體(OLED)之半透明、光散射玻璃基板的新方法及關於可由此方法獲得之基板。
OLED為光電元件,其包含夾於兩個電極(其中至少一者為半透明)之間的具螢光或磷光染料之有機層堆疊。當施加電壓於電極時,自陰極射出的電子與自陽極射出的電洞在有機層中結合,產生來自螢光/磷光層之發光。
周知來自慣用OLED之光萃取(light extraction)欠佳,大部分的光因全內反射(total internal reflection)而陷於高折射率有機層和透明導電層(TCL)中。全內反射不僅發生於高折射率TCL和下方玻璃基板(折射率為約1.5)間的邊界,亦發生於玻璃和空氣間的邊界。
據估計,在不包含任何額外萃取層的慣用OLED中,約60%自有機層發出的光陷於TCL/玻璃邊界,另20%部
分則陷於玻璃/空氣表面,且僅約20%離開OLED進入空氣中。
已經知道藉由在TCL和玻璃基板之間的光散射層降低此光捕陷(light entrapment)。此光散射層具有具高折射率(接近TCL折射率)的透明基質且含有多個折射率與基質者不同的光散射元件。此高折射率基質一般藉由熔化高折射率玻璃粒料(high index glass frit)而獲得以在低折射率玻璃基板上得到薄的高折射率琺瑯層。光散射元件可為在熔化步驟前加至玻璃粒料的固態粒子、在熔化步驟期間形成的晶體或是在熔化步驟期間形成的氣泡。
也已經知道,光萃取(out-coupling of light)之提升,係可藉由界面的紋理化(texturing),即,於玻璃和OLED的高折射率層之間的界面製造起伏(relief),例如藉由在施加及熔化高折射率玻璃粒料之前蝕刻或重疊低折射率透明基板。
此等萃取方式通常皆被稱為“內部萃取層(IEL)”,因為彼等係位於OLED基板和TCL之間。
外部萃取層(EEL),亦為本領域所周知,以類似方式作用,但係位於玻璃/空氣邊界。
本發明係屬於具透明高折射率玻璃基質(含有氣泡作為低折射率擴散元件)之內部萃取層(IEL)的領域。此具有光擴散氣泡的IEL係比具固態粒子的類似IEL有利,這是因為不會有大尺寸粒子自基質突出及在最終OLED產品中造成短路及/或內部電極漏電流(leakage current)的風
險。
但是,儘管沒有固態粒子存在,藉由簡單地於低折射率玻璃基板上熔化高折射率玻璃粒料,不易得到具有完美表面品質的擴散性琺瑯(diffusing enamel)。事實上,在熔化步驟期間形成且陷於熔融基質中的氣泡係朝向表面上升,於該處破裂和整平(level out)。但是開放或部分開放氣泡,在完全整平之前於IEL表面固化,產生像坑的表面不規則,其可具有頗尖銳的邊緣並導致內部電極漏電流(inter-electrode leakage current)及最終OLED中的針孔。
EP 2 178 343 B1揭示用於具有內部萃取層(散射層)之OLED的半透明玻璃基板,包含高折射率玻璃基質和氣泡散射元件。根據此文件,因為開放的氣泡坑(open air bubble crater),所以散射層表面沒有表面缺陷(參見[0026]至[0028],以及圖55)。但是,徹底分析此文件尤其是[0202]顯示,此僅係計算較低表層中的散射元件之不適切方法所致之人為結果。
申請人最近提出申請的南韓專利申請案第10-2013-0084314號(2013年7月17日)(在本申請案申請日時尚未公開)揭示了用於發光裝置之層壓基板(laminate substrate),具有位於低折射率玻璃基板和高折射率琺瑯間之界面處的高度互連孔隙之系統。此散射層具有極高表面品質、開放氣泡密度係低於0.1/cm2,但卻有與層壓基板邊緣接觸的水或其他流體會經由互連之孔隙而於層壓板之多數區域滲出、且經由針孔而滲入具螢光或磷
光染料之有機層的堆疊中造成對該等層之破壞的麻煩。
因此,有利地,係提出用於OLED的層壓基板,其類似於Saint-Gobain Glass France於2013年7月17日提出申請的南韓專利申請案第10-2013-0084314號中所描述者,其中於高折射率琺瑯/玻璃基板層之互連孔隙系統係置換成未彼此相連且留置於該界面(基本上沒有上升至熔融之高折射率玻璃粒料的表面)的多個個別氣泡。
申請人訝異地發現到,當玻璃粒料之施加及熔化並未直接與玻璃基板接觸而是在事先塗覆於該玻璃表面的薄金屬氧化物層上時,有大量的個別氣泡形成於熔融之高折射率粒料的較低層中,留置於下方之玻璃基板(基本上沒有上升至表面)。與此方法及產品相關之一歐洲專利申請案(EP 14177291.3)已於最近提出申請,但於本申請案申請之前尚未公開。
申請人現訝異地發現另一種方法,其中薄金屬氧化物層係塗覆於高折射率琺瑯層頂部-而不是(如於EP14177291.3中)在該琺瑯層之下。經塗覆之基板/琺瑯/金屬氧化物層壓板隨後係於約570℃燒製。燒製時,頂部金屬氧化物層的成分與下方琺瑯的成分反應,形成其內陷有複數個球形孔隙(spherical void)的薄表層。相當訝異地發現,球形孔隙(spherical void)儘管與經燒製之層的表面如此相近,卻能有利地不會上升至表面而破裂。開放或部
分開放氣泡、在完全整平之前於表面處固化,的確會產生像坑般的表面不規則,其可具有頗尖銳的邊緣並導致內部電極漏電流及最終OLED中的針孔。頗令人訝異的事實為在高折射率琺瑯之上表面層中形成的孔隙,並不會上升至其表面,因而能保證有優異的表面品質(surface quality)且避免最終OLED中之漏電流。
此外已顯示(參見圖4),於高折射率琺瑯層上塗覆及燒製(firing)此薄金屬氧化物層,能夠改善(heal)、或補救(cure)之前存在的開放氣泡表面缺陷。
本案之標的為製備用於發光裝置之層壓基板(laminate substrate)的方法,其包括至少下列五步驟:(a)提供具有折射率(於λ=550nm)為1.45至1.65的玻璃基板,(b)將具有折射率(於λ=550nm)為至少1.7之玻璃粒料(glass frit)塗覆至該玻璃基板,(c)在高於玻璃粒料之利托敦溫度(Littleton temperature)的溫度,燒製(firing)經粒料塗覆的玻璃基板,以形成第一高折射率琺瑯層(first high index enamel layer),(d)將金屬氧化物層塗覆至該第一高折射率琺瑯層,以及(e)在高於玻璃粒料之利托敦溫度(Littleton temperature)的溫度,燒製(firing)所得之經塗覆的玻璃基板,以使金屬氧化物與下方之第一高折射率琺瑯層反應、
及形成第二高折射率琺瑯層(second high index enamel layer)其具有複數個球形孔隙(spherical void)埋於第二琺瑯層之上段中接近與空氣之界面處。
本案之另一標的為可由前述方法獲得之層壓基板(laminate substrate),該層壓基板包括(i)玻璃基板,具有1.45至1.65之折射率(refractive index),(ii)高折射率玻璃琺瑯層,具有折射率(於550nm)為至少1.7,其特徵在於,有複數個球形孔隙(spherical void)埋於高折射率琺瑯層中接近其表面處,至少95%、較佳為至少99%、更佳為實質上所有之球形孔隙的直徑係顯著小於琺瑯層(enamel layer)的半值厚度(half-thickness),且係位於該高折射率琺瑯層之上半部中接近與空氣之界面處。
步驟(a)中提供之玻璃基板為礦物玻璃(mineral glass)(例如,鈉鈣玻璃(soda lime glass))之平坦的半透明或透明基板,通常具有厚度為0.1至5mm、較佳為0.3至1.6mm。其透光率(light transmission)(ISO9050標準,illuminant D65(TLD),如由ISO/IEC 10526標準所定義,考量測色標準觀測者(standard colorimetric observer)CIE 1931,如由ISO/IEC 10527所定義)較佳為儘量高且通常高於80%、較佳為高於85%或甚至高於90%。
本發明之方法的步驟(b)中,於λ=550nm之折射率為至少1.7的玻璃粒料(glass frit)係塗覆至該玻璃基板。
該玻璃粒料的折射率較佳係介於1.70和2.20之間、更佳係介於1.80和2.10之間。
高折射率玻璃粒料有利地為包含至少30重量%、較佳為至少50重量%、更佳為至少60重量%之Bi2O3。
應選擇玻璃粒料以具有熔點(利托敦點(Littleton point))為介於450℃和570℃,且應獲致折射率為1.8至2.1的琺瑯(enamel)。
較佳之玻璃粒料係具有下列組成:Bi2O3:55-75wt%
BaO:0-20wt%
ZnO:0-20wt%
Al2O3:1-7wt%
SiO2:5-15wt%
B2O3:5-20wt%
Na2O:0.1-1wt%
CeO2:0-0.1wt%
於一典型的實施態樣中,玻璃粒料(glass frit)粒子(70-80wt%)係與20-30wt%之有機媒液(organic vehicle)(乙基纖維素(ethyl cellulose)及有機溶劑)混合。所得之粒料糊(frit paste)係隨後藉由網版印刷(screen printing)或狹縫模具式塗覆(slot die coating)而施加至該玻璃基板。所得之層係藉由於120-200℃之溫度加熱而乾燥。有機黏合劑(乙基纖維素)係在350-440℃的溫度燒除(burn out)。
塗覆於玻璃基板之高折射率玻璃粒料的量通常係介於20和200g/m2之間、較佳係介於25和150g/m2之間、更佳係介於30和100g/m2之間、最佳係介於35和70g/m2之間。
經粒料塗覆(frit-coated)的玻璃基板接著係經受第一燒製(firing)步驟(步驟(c)),其中該玻璃粒料係加熱到高於該玻璃粒料之利托敦溫度(Littleton temperature)的溫度,使玻璃粒料熔化(fusion)且形成第一高折射率琺瑯層(first high index enamel layer)。此燒製步驟,即,高折射率玻璃粒料的熔化、獲得第一高折射率琺瑯層,較佳係於530℃至620℃的溫度進行、更佳為540℃至600℃。
於本發明之方法的下個步驟(步驟(d))中,係藉由任何合適之方法將金屬氧化物之薄層塗覆至第一高折射率琺瑯層上,較佳係藉由反應性(reactive)或非反應性(non-reactive)磁控濺射(magnetron sputtering)、化學氣相沈積(chemical vapor deposition)(CVD)、原子層沉積(atomic layer deposition)(ALD)或溶膠-凝膠濕式塗覆(sol-gel wet coating)。該金屬氧化物層可覆蓋第一琺瑯層的整個表面。於另一實施態樣中,僅部分的第一琺瑯層表面塗覆了金屬氧化物層。尤關注者可為以圖案化(patterned)金屬氧化物層塗覆該基板以製備具有非均勻萃取圖案(non-uniform extraction pattern)的最終層壓基板。
在塗覆金屬氧化物層之後,所得之經塗覆的玻璃基板係經受第二燒製步驟(步驟(e))。
不欲受任何理論所限,申請人認為光散射球形孔隙(light scattering spherical void)係在燒製步驟(e)期間藉由金屬氧化物與下方之第一高折射率琺瑯層的成分之間的反應所產生。該反應的具體性質尚未被完全闡明。認為O2氣體可能釋放為反應產物。大多數的球形孔隙(spherical void)並非就是熔化-固化(fusion-solidification)步驟期間陷於玻璃粒料中的氣泡(如於EP 2 178 343 B1中所述),而是燒製步驟期間產生的氣泡。
實際上,申請人觀察到塗覆有金屬氧化物層之第一琺瑯層的區域內的球形孔隙(spherical void)密度係遠高於未塗覆之區域。
金屬氧化物層的厚度並無特定下限,只要其能提供足夠之反應成分(reactive component)以在第二高折射率琺瑯層的上半部中產生顯著量之球形孔隙(spherical void)即可。數奈米之金屬氧化物層僅證明能引發形成所想要的球形孔隙。金屬氧化物層較佳應夠薄以能在第二燒製步驟期間藉由與下方高折射率琺瑯的反應而完全分解(break down)。
金屬氧化物層之厚度較佳為5至60nm、更佳為10至40nm、甚至更佳為15至30nm。
本申請案申請時,申請人已以實驗顯示至少三種金屬氧化物,即,TiO2、Al2O3、ZrO2,使得形成該球形孔隙(spherical void)。在不悖離本發明之精神下,習此技藝之人士可容易地將此等金屬氧化物換成不同的金屬氧化物例
如Nb2O5、HfO2、Ta2O5、WO3、Ga2O3、In2O3及SnO2、或彼等之混合物,以完成申請人之實驗工作並發掘適用於本發明之方法的其他金屬氧化物。
金屬氧化物因此較佳係選自下列所組成之群組:TiO2、Al2O3、ZrO2、Nb2O5、HfO2、Ta2O5、WO3、Ga2O3、In2O3、SnO2、及彼等之混合物。
於燒製步驟(e)中,基板係再被加熱到高於玻璃粒料之利托敦溫度(Littleton temperature)的溫度,使金屬氧化物的成分與下方之高折射率琺瑯層的成分反應,且於此反應區域中形成球形孔隙(spherical void)。於最終之固化的琺瑯塗覆中,一般無法清楚區分原先的金屬氧化物層與玻璃粒料層。最有可能的是金屬氧化物層係被第一琺瑯層所解(digest),就地產生具稍微不同組成之熔化的琺瑯。因此無法具體指明在最終之層壓板中之此兩層的各自厚度。
固化之琺瑯層(稱為“第二高折射率琺瑯層(second high index enamel layer)”,包含埋於其中的複數個球形孔隙(散射元件(scattering element)))的整體厚度,較佳係介於3μm和25μm之間、更佳係介於4μm和20μm之間、最佳係介於5μm和15μm之間。
本發明最令人訝異的態樣中之一者為觀察到於第二燒製步驟(步驟(e))期間形成的氣泡不會在熔化玻璃相(molten glass phase)中朝其表面上升,而是看來會留在略低於與大氣之界面的位置。此散射元件之“留下(holding down)”使固化之高折射率琺瑯具極佳表面品質(surface
quality),而不會有因固化之開放泡泡所致之像坑的凹陷(crater-like recess)。
然而,為有效避免球形孔隙上升至第二高折射率琺瑯層的表面,步驟(e)的燒製溫度不應過高且燒製步驟的時程不宜過長。
燒製步驟(e)的時程較佳係介於3和30分鐘之間、更佳係介於5和20分鐘之間。步驟(e)的燒製溫度應介於530℃和620℃之間、更佳係介於540℃和600℃之間。燒製溫度之選擇係取決於高折射率玻璃粒料的利托敦溫度(Littleton temperature),且較佳為比該高折射率玻璃粒料的利托敦溫度(Littleton temperature)高約40至80℃。
毋須贅言,本發明中所用之高折射率玻璃粒料及由此所得之琺瑯(enamel)應較佳為實質上沒有固體散射粒子如結晶SiO2或TiO2粒子。此等粒子常作為內部萃取層(internal extraction layer)的散射元件(scattering element),但須要額外的平坦化層(planarization layer),因而非所欲地增加萃取層的總厚度。
如前文已解釋,在燒製步驟期間形成的球形孔隙(spherical void)並非隨機分佈於第二高折射率琺瑯層的整個厚度,而是主要位於“上”半部,即,接近該琺瑯層與空氣的界面。為了完全埋在琺瑯層中,球形孔隙當然必須顯著小於琺瑯層的厚度。至少95%、較佳為至少99%、更佳為實質上所有的球形空氣孔隙係具有小於琺瑯層的半值厚度(half-thickness)之直徑,且係位於高折射率琺瑯層之上
半部中、接近其與大氣之界面。“位於高折射率琺瑯層之上半部中”一詞意指至少80%的孔隙體積係位在琺瑯層之中心平面(median plane)以上。
球形孔隙(spherical void)之平均等效球直徑(average equivalent spherical diameter)較佳為0.2μm至8μm、更佳為0.4μm至4μm、最佳為0.5μm至3μm。
球形孔隙係隨機地分佈在對應於事先塗覆有金屬氧化物層之表面的全區域。為有效地散射從含有螢光或磷光染料之有機層的堆疊所發出的光,球形孔隙的密度較佳為介於104和25.106(每mm2)、更佳為介於105和5.106(每mm2)。
從垂直於基板之任意平面(general plane)的方向觀之(投影視圖(projection view)),球形孔隙(spherical void)較佳係佔事先以金屬氧化物覆蓋之區域的表面之至少20%、更佳為至少25%,且最多佔該表面之80%、更佳為最多70%。
如可由分別出示根據本發明之層壓基板(laminate substrate)的透視圖與剖視圖之圖2及圖3所見,幾乎所有的球形孔隙(spherical void)係隨機地列於最終琺瑯層的上三分之一中,因而形成某種個別孔隙之單層,“浮(floating)”於該表面下方但不與其接觸。該孔隙可非常接近彼此或甚至彼此接觸但並未彼此相連。因此,有效地阻礙從本發明層壓基板(laminate substrate)周圍進入之流體(例如水或其他溶劑(呈液體或氣體形式))的滲出
(percolation)。因此,由本發明之層壓基板所製造的OLED對於水或溶劑的敏感度遠小於由南韓專利申請案第10-2013-0084314號中所述之層壓基板所製造者。
本發明之層壓基板(laminate substrate)要作為用於製造底部發光型OLED(bottom emitting OLED)之半透明基板。底部發光型OLED包含帶有半透明電極(通常是陽極)的半透明基板、以及光反射電極(light reflecting electrode)(通常是陰極)。從發光有機層之堆疊所發出的光係直接經由半透明陽極和基板發射或者先藉陰極反射朝向且通過半透明陽極和基板。
在層壓該發光有機層堆疊(light emitting organic layer stack)之前,透明導電層(電極層)必須因此塗覆於內部萃取層頂部。在一較佳實施態樣中,本發明之層壓基板因而進一步包含在高折射率琺瑯層上的透明導電層(transparent electro-conductive layer),此導電層較佳係直接與琺瑯層接觸或者係塗覆於中間層(例如障壁層(barrier layer)或保護層)上。
在一較佳實施態樣中,本發明之方法因而進一步包括另一步驟:將透明導電層(TCL)塗覆於高折射率琺瑯層上。此層較佳為透明導電氧化物,如ITO(銦錫氧化物)。此TCL之形成係可根據嫻於此技術者熟知的慣用方法(例如磁控濺射(magnetron sputtering))進行。
1‧‧‧玻璃基板
2‧‧‧金屬氧化物層
3‧‧‧玻璃粒料
4‧‧‧第一高折射率琺瑯層
5‧‧‧第二高折射率琺瑯層
6‧‧‧球形孔隙
7‧‧‧界面
8‧‧‧透明導電層
圖1係流程圖,出示製備本發明之層壓基板(laminate substrate)的方法。
圖2係掃描式電子顯微鏡(SEM)照片,出示在燒製步驟(e)之後的本發明之層壓基板的截面、頂面圖。
圖3係掃描式電子顯微鏡(SEM)照片,出示根據本發明之層壓基板的截面圖。
圖4係出示層壓基板之四個俯視圖:具有之前存在的開放氣泡表面缺陷(open-bubble surface defect)、在藉由塗覆及燒製薄金屬氧化物層進行補救(curing)之前及之後。
圖5係出示根據以下實施例製備之層壓基板的俯視圖(top view)及截面圖(cross-sectional view)。
圖1中,首先於步驟(a)中提供平坦透明之玻璃基板1。在步驟(b)中,接著將高折射率玻璃粒料3塗覆至此基板的一側,係藉由例如網版印刷(screen printing)包含該玻璃粒料及有機介質(聚合物和有機溶劑)的糊。在下個步驟(步驟(c))中,將所得之經玻璃粒料塗覆的基板加熱至足以將該粒料熔成連續之高折射率琺瑯層4的溫度。隨後藉由例如磁控濺射(magnetron sputtering),以金屬氧化物2塗覆此第一高折射率琺瑯層4。
所得之於第一高折射率琺瑯層4上帶有金屬氧化物層2的基板係接著經受第二燒製步驟(步驟(e))。於此最後加熱步驟期間,由金屬氧化物和第一高折射率琺瑯層4之
間的反應形成球形孔隙(spherical void)6,產生第二高折射率琺瑯層(second high index enamel layer)5,其含有(在其與大氣之界面7下方)一排細微之球形孔隙6。該球形孔隙頗為接近該第二高折射率琺瑯層5的表面,但並未上升至此層的表面。接著於步驟(f)中將透明導電層6塗覆至第二高折射率琺瑯層5的完美平順表面。
於圖2的SEM照片可見到在琺瑯層之表面下方的那排小球形孔隙,還有此琺瑯層的高表面品質(surface quality)。
於圖3的SEM照片,黑色的玻璃基板係被高折射率琺瑯之淡灰層所覆蓋,對應於圖1之第二高折射率層5。不同尺寸之球形孔隙的單層係完全埋於其中且位在與空氣(上面的黑色區域)之界面相近處但明顯在該界面下方。
所示之層壓基板尚未含有透明導電層。可以看到高折射率琺瑯層之表面係完美平順(smooth)且無像坑的表面不規則(crater-like surface irregularity)。
於圖4的第一排可看到在本發明的燒製步驟(c)後由高折射率琺瑯層中之固化的破裂氣泡所致之兩表面缺陷。接著在薄TiO2層之塗覆及燒製10分鐘(於570℃)後再次拍攝相同的缺陷。缺陷皆仍略可見之但其邊緣之清晰度已完全消失。有發生對該等表面缺陷之改善(healing)。
0.7mm鈉鈣玻璃片(soda lime glass sheet),以含有75
重量%之高折射率玻璃粒料(Bi2O3-B2O3-ZnO-Al2O3-SiO2)及25重量%之有機介質(乙基纖維素(ethyl cellulose)及有機溶劑)的糊進行網版印刷(screen print),並進行乾燥步驟(10分鐘,於150℃)。
基板接著於570℃燒製約10分鐘,得到厚度為12μm的高折射率琺瑯層。
接著利用溶膠凝膠沉積(sol-gel deposition)以TiO2前驅物(precursor)塗覆所得之經琺瑯塗覆的玻璃片,且於560℃燒製約10分鐘,得到含有複數個球形孔隙(接近表面)的高折射率琺瑯層。
球形孔隙之平均尺寸以及涵蓋率(coverage rate)(被球形孔隙所佔之經TiO2塗覆表面的面積百分比)係藉由影像分析(image analysis)來量測。下表顯示球形孔隙之平均尺寸(mean size)、所得基板之涵蓋率(coverage rate)及霧度(haze ratio),與進行相同處理與分析但無TiO2塗覆步驟之同樣基板相比較。
負對照組之高折射率琺瑯層並無球形孔隙位於琺瑯層
頂部。
此等實驗數據清楚顯示於琺瑯層頂部的球形孔隙係來自於金屬氧化物層與覆蓋之高折射率玻璃粒料之間的交互作用。
圖5出示對應於表1之樣品的俯視圖(左)及截面圖(右)。
Claims (10)
- 一種製備用於發光裝置之層壓基板(laminate substrate)的方法,其包括至少下列步驟:(a)提供具有於550nm之折射率為介於1.45和1.65之間的玻璃基板(1),(b)將具有於550nm之折射率為至少1.7之玻璃粒料(glass frit)(3)塗覆至該玻璃基板(1),該玻璃粒料包含至少30重量%之Bi2O3,(c)在高於玻璃粒料之利托敦溫度(Littleton temperature)且介於530℃和620℃之間的溫度,燒製(firing)所得之經粒料塗覆的玻璃基板,以形成第一高折射率琺瑯層(4),(d)將金屬氧化物層(2)塗覆至該第一高折射率琺瑯層,該金屬氧化物係選自下列所組成之群組:TiO2、Al2O3、ZrO2、Nb2O5、HfO2、Ta2O5、WO3、Ga2O3、In2O3和SnO2,及彼等之混合物,以及(e)在高於玻璃粒料之利托敦溫度且介於530℃和620℃之間的溫度,燒製(firing)所得之經塗覆的玻璃基板,以使金屬氧化物(2)與下方之該第一高折射率琺瑯層(4)反應,且形成第二高折射率琺瑯層(5),其具有複數個球形孔隙(spherical void)(6)埋於該第二高折射率琺瑯層(5)之上段中接近與空氣之界面處。
- 如申請專利範圍第1項之方法,其中,該金屬氧化物層之厚度為介於5和60nm之間。
- 如申請專利範圍第1項之方法,其中,該玻璃粒料之折射率係介於1.70和2.20之間。
- 如申請專利範圍第1項之方法,其中,該玻璃粒料包含至少50重量%之Bi2O3。
- 如申請專利範圍第1項之方法,其中,該燒製步驟(c)及(e)係在介於540℃和600℃之間的溫度進行。
- 如申請專利範圍第1項之方法,其進一步包括(f)將透明導電層(TCL)(8)塗覆於該第二高折射率琺瑯層(5)。
- 一種可由如申請專利範圍第1至6項中任一項之方法獲得之層壓基板,其包括(i)玻璃基板(1),具有介於1.45和1.65之間之折射率,(ii)高折射率玻璃琺瑯層(5),具有於550nm之折射率為至少1.7,且包含至少30重量%之Bi2O3,其特徵在於,有複數個球形孔隙(6)埋於高折射率琺瑯層(5)中接近其表面處,至少95%、較佳為至少99%、更佳為實質上所有之球形孔隙係具有顯著小於高折射率琺瑯層(5)之半值厚度(half-thickness)的直徑且係位於該高折射率琺瑯層之上半部中接近與空氣之界面(7)處。
- 如申請專利範圍第7項之層壓基板,其中,該球形孔隙之平均等效球直徑(average equivalent spherical diameter)為介於0.2μm和8μm之間。
- 如申請專利範圍第7或8項之層壓基板,其中,第二高折射率琺瑯層(5)之厚度係介於3μm和25μm之間。
- 如申請專利範圍第7或8項之層壓基板,其進一步包括(iii)透明導電層(8),係於高折射率琺瑯層(5)上。
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